EP0451785B1 - Pigment d'aluminium et procédé de production - Google Patents

Pigment d'aluminium et procédé de production Download PDF

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Publication number
EP0451785B1
EP0451785B1 EP91105605A EP91105605A EP0451785B1 EP 0451785 B1 EP0451785 B1 EP 0451785B1 EP 91105605 A EP91105605 A EP 91105605A EP 91105605 A EP91105605 A EP 91105605A EP 0451785 B1 EP0451785 B1 EP 0451785B1
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EP
European Patent Office
Prior art keywords
pigment
grinding
aluminium
aluminum
aluminum pigment
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EP91105605A
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German (de)
English (en)
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EP0451785B2 (fr
EP0451785A1 (fr
Inventor
Yasunobu Imasato
Mikio Suzuki
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Asahi Kasei Metals Ltd
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Asahi Kasei Metals Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/62—Metallic pigments or fillers
    • C09C1/64—Aluminium
    • C09C1/644—Aluminium treated with organic compounds, e.g. polymers
    • C09C1/646—Aluminium treated with organic compounds, e.g. polymers concomitant with mechanical comminution, shaping or abrasion of the particles
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/62—Metallic pigments or fillers
    • C09C1/64—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S75/00—Specialized metallurgical processes, compositions for use therein, consolidated metal powder compositions, and loose metal particulate mixtures
    • Y10S75/954—Producing flakes or crystals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12014—All metal or with adjacent metals having metal particles

Definitions

  • the present invention relates to an aluminum pigment and process for producing the same.
  • the present invention relates to an aluminum pigment used in high-quality metallic paints including, for example, high-quality metallic paints for automobile bodies and automotive parts, metallic paints for automobile repairing, metallic paints for household electric appliances, high-quality metallic paints for industrial uses and the like, high-quality metallic printing inks for gravure printing, offset printing, screen printing and the like for plastics and for other uses.
  • the present invention relates to an improved aluminum pigment capable of giving a higher than conventional reflectivity and a very high substrate-hiding power to paint films, prints, plastic films and other materials described above by ordinary application methods.
  • Aluminum pigments are generally characterized by their unique metallic impression not possessed by other pigments and their excellent substrate-hiding power and have been widely used for the above-mentioned purposes.
  • paints which give a soft metallic tone.
  • all of these paints contain a special pigment utilizing a light-interfering action (this special pigment is hereinafter referred to as a pearl pigment).
  • a pearl pigment however, has little or no substrate-hiding power because it is generally transparent and transmits light.
  • an undercoating step has been necessary prior to the application of a paint containing a pearl pigment in order to hide the substrate.
  • attempts have been made to eliminate the undercoating step by making a coating by mixing the pearl pigment with an aluminum pigment.
  • This coating however, has a serious problem in that the mixing impairs the soft metallic tone characterizing the pearl pigment. The problem is caused by the aluminum pigment which is mixed with the pearl pigment.
  • Two technical factors are necessary in order to impart satisfactory hiding power without impairing the soft metallic tone characterizing the pearl pigment.
  • One technical factor is to minimize the amount of the aluminum pigment to be mixed with the pearl pigment. To achieve this, an aluminum pigment capable of imparting a very high hiding power when used in a small amount is required.
  • the other technical factor is that the aluminum pigment to be mixed with the pearl pigment must have a high reflectivity.
  • the soft metallic tone characterizing the pearl pigment is given by the light-interfering action possessed by the pearl pigment.
  • the pearl pigment itself has a very low or substantially no light-reflecting ability because the pigment transmits most light.
  • the light-reflecting ability is possessed by the aluminum pigment mixed into the pearl pigment.
  • the soft metallic tone of the pearl pigment is not obtained and only a black opaque color tone or appearance having a low commercial value is obtained.
  • an aluminum pigment having a high hiding power and a high light reflectivity is required.
  • an aluminum pigment of higher hiding power has a lower reflectivity. Therefore, it has been difficult to provide an aluminum pigment excellent in both hiding power and reflectivity.
  • EP-A-0 305 158 describes an aluminium flake pigment suitable to use in a paint.
  • the ratio of the average thickness of the flakes to the average diameter of the flakes is reported to be from 0.025 : 1 to 0.3 : 1 and the ratio of the water covering area of the flakes to the specific surface area of the flakes is from 0.18 : 1 to 0.4 : 1.
  • US-A-3,901,688 relates to aluminium flake powder having high specular reflectivity.
  • Said powder is produced by wet ball milling aluminium powder in the presence of a lubricant using a volume ratio of grinding balls to powder of at least 15 : 1 and a volume ratio of grinding balls to milling liquid which is preferably substantially equal.
  • the present inventors studied the relation between the basic properties and optical properties of aluminum pigment and, as a result, discovered that an aluminum pigment can exhibit a high hiding power and a very high reflectivity by controlling the ratio of specific surface area to water coverage and the flakiness of the aluminum pigment. This finding has led to the present invention.
  • the present invention provides an aluminum pigment having a water coverage of 2.5-5.0 m 2 /g, a ratio of specific surface area in m 2 /g to water coverage in m 2 /g of 5.0 or less and a flakiness dso/t of 90 or more wherein dso is the average particle diameter of the pigment in /1.m and t is the average thickness of the pigment in /1.m to achieve a higher than conventional reflectivity and a very high hiding power.
  • the present invention provides an aluminum pigment which, when used together with a pearl pigment, does not impair the soft metallic tone of the pearl pigment.
  • One pearl pigment which provides a soft metallic tone is a flaky mica powder coated with a metal oxide such as Ti0 2 or the like.
  • These pearl pigments include those, when orientated in a paint film, giving a pearly luster by multiple reflection of light, those producing color by interference of light due to a thick metal oxide layer, and those further containing a coloring agent.
  • a pearl pigment is EXTERIOR MEARLINO produced by the MEARL Corporation. The product comes in various colors such as, for example, Bright White, Bright Gold, Brass, Europearl, Bright Bronze, Bright Orange, Fine Pearl, Fine Gold and Fine Brass.
  • the type of pearl pigment is not particularly restricted in the present invention.
  • the embodiments of the aluminum pigment of the present invention are not restricted only to their combined use with a pearl pigment.
  • the present aluminum pigment may be used alone or may be used in combination with a transparent organic pigment.
  • the high reflectivity and hiding power of the aluminum pigment are very advantageous properties and can greatly contribute to the enhancement of commercial value.
  • the ratio of specific surface area to water coverage referred to in the present invention can be measured by the following method.
  • the specific surface area in m 2 /g is an area (S1) per 1 g of an aluminum pigment as calculated from the amount of absorbed nitrogen measured by the BET method; water coverage in m 2 /g is an area (S2) per 1 g of an aluminum pigment as measured by the method specified in DIN 55923; the ratio of specific surface area to water coverage can be determined as S1/S2.
  • a specific surface area tester (Flowsorb 2,300 manufactured by Shimadzu Corp.) was used to measure specific surface area.
  • the flakiness referred to in the present invention is represented by dso/t wherein the dso, in ⁇ m, is the average particle diameter of an aluminum pigment and t, in ⁇ m, is the average thickness of the aluminum pigment.
  • the average particle diameter (dso) can be measured by a laser method (SK laser PRO 7,000 manufactured by Seishin Kogyo K.K.), and the average thickness (t) can be determined by the following formula:
  • the novel aluminum pigment according to the present invention has a water coverage of 2.5-5.0 m 2 /g, a ratio of specific surface area to water coverage of 5.0 or less and a flakiness dso/t of 90 or more wherein dso is the average particle diameter of the pigment in ⁇ m and t is the average thickness of the pigment in /1.m.
  • the ratio of specific surface area to water coverage is 5.0 or less and the flakiness is 100 or more. More preferably, the ratio of specific surface area to water coverage is 4.0 or less and the flakiness is 100 or more.
  • the ratio of specific surface area to water coverage is greater than 5.0 or the flakiness is less than 90, there occurs a sharp reduction in reflectivity of the aluminum pigment.
  • the flakiness is larger than 200, the particles of aluminum pigment bend easily and such a flakiness is not preferred.
  • the novel aluminum pigment of the present invention has a water coverage of 2.5-5.0 m 2 /g.
  • the water coverage is smaller than 2.5 m 2 /g, the desired hiding power is not obtained.
  • the water coverage is larger than 5.0 m 2 /g, a sharp reduction in reflectivity occurs.
  • the specific surface area can be appropriately set based on the ratio of water coverage but is preferably 5-25 m 2 /g in view of reflectivity.
  • the reflectivity of the aluminum pigment can be determined by forming a conventional silver metallic film containing only an aluminum pigment and measuring the L value of the film using a color computer.
  • the concentration of aluminum pigment was set at 10 PHR and a paint film was formed by an applicator adjusted to give a film thickness (as dried) of 35-40 /1.m.
  • the film preparation is not restricted to this practice.
  • an aluminum pigment was incorporated into a commercially available acryl clear (Acrylic 2026GL Clear manufactured by Kansai Paint Co., Ltd.) at a concentration of 10 PHR to prepare a silver metallic paint.
  • the paint was coated on an art paper using an applicator to form a film thereon.
  • the film was dried at room temperature for 24 hours and the dried film was measured for L value using a SM color computer, Model SM-4 manufactured by Suga Shikenki K.K.
  • the silver metallic film containing only the aluminum pigment of the present invention gives a significantly improved reflectivity (L value) as compared with the film containing a conventional aluminum pigment.
  • the aluminum pigment of the present invention gives a L value of 75-87%, preferably 77-87%.
  • hiding power refers to the hiding power of a silver metallic paint containing only an aluminum pigment and can be measured as follows.
  • An aluminum pigment is incorporated into an acrylic clear varnish (Acrylic 2026GL Clear manufactured by Kansai Paint Co., Ltd.) at a concentration of 5 HPR to prepare a silver metallic paint.
  • This paint is coated on a hiding chart (approved by Japan Paint Inspecting Association) using an applicator, to form films of different thicknesses.
  • the films are dried at room temperature for 24 hours.
  • Each dried film is measured for diffuse reflectivities on white and black portions using a SM color computer, Model SM-2, manufactured by Suga Shikenki K.K.
  • the ratio of diffuse reflectivity (Rb) of the black portion to diffuse reflectivity (Rw) of the white portion i.e. Rb/Rw
  • Rb/Rw diffuse reflectivity
  • This hiding film thickness is the hiding power of an aluminum pigment.
  • a smaller hiding film thickness indicates a higher hiding power.
  • the aluminum pigment of the present invention gives a small hiding film thickness of less than 20 ⁇ m.
  • the aluminum pigment of the present invention has a high reflectivity and a very high hiding power. Therefore, the present aluminum pigment, as compared with conventional aluminum pigments, gives a large value when the L value of silver metallic paint film is divided by the hiding film thickness. This differentiates the aluminum pigment of the present invention from conventioal aluminum pigments.
  • the aluminum pigment of the present invention contains coarse particles with a diameter of 44 /1 .m or more in an amount of 0.1% or less when measured as screening residue, and has an average particle diameter (d so ) of 5-25 ⁇ m when measured by a laser method (SK laser PRO 7,000) and accordingly has a sharp particle distribution.
  • the amount of coarse particles of 44 /1 .m or more, when measured as screening residue, is larger than 0.1%, lumps are seen in the film formed.
  • the amount of coarse particles is preferably 0.05% or less.
  • the average particle diameter (dso) is smaller than 5 ⁇ m, the resulting film gives a low reflectivity.
  • the average particle diameter (dso) is larger than 25 ⁇ m, the resulting film gives too strong of a reflection from the aluminum particles, impairing the soft metallic tone.
  • the average particle diameter (d so ) is preferably 7-20 /1.m.
  • the aluminum pigment of the present invention contains at least one fatty acid derivative selected from fatty acids (e.g. oleic acid, behenic acid, arachic acid, stearic acid, palmitic acid, myristic acid, lauric acid, caproic acid, caprylic acid or capric acid; their metal salts; aliphatic amines (e.g. laurylamine, stearylamine); aliphatic alcohols (e.g. stearyl alcohol, oleyl alcohol); fatty acid amides (e.g. stearamide, oleamide); etc., in order to prevent the agglomeration of pigment.
  • fatty acids e.g. oleic acid, behenic acid, arachic acid, stearic acid, palmitic acid, myristic acid, lauric acid, caproic acid, caprylic acid or capric acid
  • metal salts e.g. laurylamine, stearylamine
  • aliphatic alcohols
  • the amount of fatty acid derivative is 0.2-10%, preferably about 0.5-5% based on the amount of aluminum pigment. This amount can be measured as that of the fatty acid derivative soluble in solvent, based on JIS K 5910 5.7. When the amount is smaller than 0.2%, the aluminum pigment causes agglomeration with the passage of a time. When the amount is larger than 10%, the formed film has a low strength.
  • One preferred process for producing an aluminum pigment of the present invention is as follows. Using a media agitating mill, grinding of aluminum was effected at a ratio of grinding ball weight to aluminum weight of 33-100, a ratio of grinding solvent weight to aluminum weight of 2.6-10.0, and a maximum grinding energy per each grinding ball of 10- 6 joule or less calculated as the kinetic energy of the ball at the front of each agitating arm.
  • the kinetic energy per grinding ball at the front of each agitating arm is preferably in the range of 10- 9 to 10- 6 joule.
  • the energy is smaller than 10- 9 joule, the time required for grinding is long.
  • the energy is larger than 10- 6 joule, significant reduction in reflectivity is seen.
  • the kinetic energy for one ball at the front of each agitating arm of the mill is more preferably in the range of 10- 8 to 10- 7 joule.
  • the media agitating mill is considered to be suitable because it allows easy adjustment of the kinetic energy for one ball at the front of each agitating arm of the mill at 10- 6 joule or less.
  • the aluminum pigment of the present invention can be produced by grinding at said kinetic energy for one ball at the front of each agitating arm of the mill or at a lower energy for a greater number of hours.
  • grinding occurs at a ratio of grinding ball weight to aluminum weight and a ratio of grinding solvent weight to aluminum weight, in each of the above-mentioned ranges, longer grinding time allows the resulting aluminum pigment to have a higher hiding power but a significantly reduced reflectivity. Therefore, an excessively long time is not preferred. This phenomenon is presumed to result from a nonhomogeneous state inside the mill.
  • the aluminum used in the present invention includes an atomized powder obtained by an atomization method, a foil powder obtained from an aluminum foil or the like, a waste foil, etc.
  • a preferred aluminum powder has a particle diameter of 0.1 mm or less, more preferably 100 ⁇ m or less, even more preferably 20 ⁇ m or less.
  • the aluminum purity of the aluminum powder is preferably 99.0% or more, more preferably 99.5% or more.
  • the grinding aid used is not particularly restricted, and there can be mentioned those conventionally used, such as higher fatty acids (e.g. lauric acid, myristic acid, palmitic acid, stearic acid, arachic acid, behenic acid); higher unsaturated fatty acids (e.g. oleic acid); higher aliphatic amines (e.g. stearylamine); higher aliphatic alcohols (e.g. stearyl alcohol, oleyl alcohol); higher fatty acid amides (e.g. stearamide, oleamide); and metal salts of higher fatty acids (e.g. aluminum stearate, aluminum oleate).
  • higher fatty acids e.g. lauric acid, myristic acid, palmitic acid, stearic acid, arachic acid, behenic acid
  • higher unsaturated fatty acids e.g. oleic acid
  • higher aliphatic amines e.g. stearylamine
  • the grinding aid is used in an amount of preferably 0.2-10% based on the amount of aluminum.
  • aluminum particles cause agglomeration due to the shortage of the grinding aid when the specific surface area of aluminum particles has been increased by grinding.
  • the grinding aid reduces the strength of the film formed.
  • the amount of the grinding aid is more preferably 0.5-5%.
  • the grinding solvent has no particular restriction. Conventional hydrocarbon solvents such as mineral spirits, solvent naphtha and the like can be used. Solvents of the alcohol type, ether type, ketone type, ester type and others can be used.
  • the grinding balls can be steel balls, stainless steel balls, glass balls, alumina balls, or other balls conventionally used.
  • the grinding balls have the appropriate diameter depending upon their specific gravity. It is possible to use grinding balls having two or more diameters, in combination.
  • the material of the grinding balls need not be particularly restricted, but steel is generally used in view of economy and quality.
  • the steel balls When steel balls are used in view of the desired range of grinding energy, the steel balls preferably have diameters of 5.0 mm or less, more preferably diameters of less than 3.2 mm.
  • the grinding temperature is not restricted particularly but is preferably 15-60 ° C. A grinding temperature lower than 15 ° C requires a large amount of a cooling medium and is not preferred. A grinding temperature higher than 60 ° C has increased risk of flaming of the solvent, etc. and is not preferred.
  • the media agitating mill used in the present invention has a structure, for example, shown in Fig. 2.
  • a fixed container 1 is provided, at the outer circumference, with a jacket 2 through which water or hot water is passed for temperature control during grinding.
  • several agitating arms 3 of round rod type are fitted to a shaft perpendicularly thereto to form an agitator 4 capable of rotating at a desired speed of 0-500 rpm.
  • the diameter, length and number of the agitating arms of round rod type vary by the size of the container 1.
  • a cover 5 is provided on the top of the container 1 as necessary.
  • the grinding energy can be controlled by the grinding balls and the rotation of the agitator.
  • the grinding energy is determined by the arm diameter and the rotation of the agitator.
  • the arm diameter is substantially determined by the capacity of the media agitating mill, but the rotation is optional.
  • the rotation required for obtaining a grinding energy suitable for use in the present invention cannot be specified because the rotation differs depending upon the size of the container 1, but the speed at the front or free end of an agitating arm of the round rod type is preferably 3 m/sec or less.
  • the aluminum pigment in which the aluminum has a flaky shape is taken out of the mill as a slurry and passed through a wet screen, which differs depending upon the application of final pigment, to remove coarse particles.
  • the resulting slurry is passed through a filter (e.g. filter press) to remove excessive solvent to obtain the aluminum pigment in a paste form.
  • the above materials were agitated at 200 rpm for 3 hours. After the completion of the agitation, the slurry in the mill was washed out with 10 t of mineral spirits and passed through a vibrating screen to remove coarse particles. The resulting slurry was passed through a filter to remove excessive solvent to obtain an aluminum pigment cake. Mineral spirits and oleic acid (1% relative to the nonvolatile content) were added to this aluminum pigment cake to prepare an aluminum pigment paste having a nonvolatile content of 65%.
  • the aluminum pigment had the following properties. This aluminum pigment meets the requirements of the present invention.
  • the aluminum pigment of the present invention showed significant improvement in reflectivity (L value) and improvement of about two times in hiding power, as compared with the conventional aluminum pigment.
  • Example 2 Aluminum pigments (samples 2-10) were prepared under the conditions shown in Table 1. The total weight of grinding balls was maintained constant (16.5 kg).
  • the samples 2-7 of the present invention showed significant improvements in the L value of paint film and hiding power, as compared with the samples 8-10 of Comparative Examples 1 to 3 and MC-808.
  • Example 2 The sample 2 obtained in Example 2 and a pearl pigment (EXTERIOR MEARLINO Fine Pearl manufactured by The Meal Corporation) were incorporated into an acryl clear pigment so that each pigment concentration became 5 PHR, whereby a paint was prepared.
  • the paint was coated on a hiding chart (meeting JIS K 5400 and approved by Japan Paint Inspecting Association) using an applicator of 6 mil, to form a film of 20 u, in thickness. The film was dried at room temperature for 24 hours.
  • the paint film using the sample 2 of the present invention had a soft metallic tone characteristic of pearl pigments and hid the substrate at a hiding film thickness of 9 ⁇ m.
  • the paint film using MC-808 had a black opaque tone and did not hide the substrate.
  • Example 1 35 kg of steel balls of 3/16 inches in diameter, 750 g of an atomized aluminum powder having an average particle diameter of 10 ⁇ m, 2.15 kg of mineral spirits and 7.5 g of stearylamine were fed into a ball mill made of iron. The ball mill was operated at 58 rpm for 3 hours. After completion of the operation, the slurry in the ball mill was washed out with 10 t of mineral spirits. Subsequently, the procedure of Example 1 was used to obtain a sample 11. The operating conditions and evaluation results are shown in Tables 1 and 2.
  • the samples 2 to 7 of the present invention showed significant improvements in L value of the resultant paint films.
  • the present invention provides an aluminum pigment having a high hiding power and a high light reflectivity.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)
  • Powder Metallurgy (AREA)

Claims (13)

1. Pigment d'aluminium ayant une couverture d'eau de 2,5-5,0 m2/g, un rapport de l'aire superficielle spécifique en m2/g à la couverture d'eau en m2/g de 5,0 ou moins et un coefficient de formation de paillettes dso/t de 90 ou plus, où dso est le diamètre moyen d'une particule du pigment en µm et t est l'épaisseur moyenne du pigment en um.
2. Pigment d'aluminium selon la revendication 1 ayant un coefficient de formation de paillettes de 100 à 200.
3. Pigment d'aluminium selon la revendication 1 ou la revendication 2 ayant une réflectivité comprise entre 75% et 87%.
4. Pigment d'aluminium selon l'une quelconque des revendications 1 à 3 ayant une épaisseur du film couvrant de moins de 20 um.
5. Pigment d'aluminium selon l'une quelconque des revendications 1 à 4 ayant une quantité de particules grossières d'un diamètre de 44 µm ou plus de 0,1% ou moins et un diamètre moyen de particules d50 de 5 - 25 um.
6. Pigment d'aluminium selon l'une quelconque des revendications 1 à 5 contenant de plus un dérivé d'acide gras.
7. Pigment d'aluminium selon l'une quelconque des revendications 1 à 6 contenant également un pigment en perle.
8. Pigment d'aluminium selon l'une quelconque des revendications 1 à 7 contenant également un pigment organique transparent.
9. Procédé de production d'un pigment d'aluminium qui consiste à broyer de l'aluminium en utilisant un broyeur a agitation à un rapport du poids des billes de broyage au poids de l'aluminium de 33 à 100, un rapport du poids du solvant de broyage au poids de l'aluminium de 2,6 à 10,0 et une énergie cinétique de 10-6 joule ou moins pour une bille à l'avant de chaque bras d'agitation du broyeur.
10. Procédé selon la revendication 9 où on utilise un auxiliaire de broyage.
11. Procédé selon la revendication 10 où la quantité de l'auxiliaire de broyage est de 0,2 à 10% en se basant sur la quantité d'aluminium.
12. Procédé selon la revendication 9 où les billes de broyage dans lesdits broyeurs sont en acier, en acier inoxydable, en verre ou en alumine.
13. Procédé selon la revendication 12 où on utilise des billes d'acier ayant un diamètre de 5,0 mm ou moins.
EP91105605A 1990-04-11 1991-04-09 Pigment d'aluminium et procédé de production Expired - Lifetime EP0451785B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP94161/90 1990-04-11
JP2094161A JP2575516B2 (ja) 1990-04-11 1990-04-11 アルミニウム顔料

Publications (3)

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EP0451785A1 EP0451785A1 (fr) 1991-10-16
EP0451785B1 true EP0451785B1 (fr) 1995-06-28
EP0451785B2 EP0451785B2 (fr) 1999-03-03

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US (1) US5127951A (fr)
EP (1) EP0451785B2 (fr)
JP (1) JP2575516B2 (fr)
KR (1) KR940005837B1 (fr)
CA (1) CA2039949C (fr)
DE (1) DE69110729T3 (fr)

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ATE146509T1 (de) * 1992-07-23 1997-01-15 Silberline Ltd Metallpulverpigment
GB2292744B (en) * 1994-08-15 1997-10-15 Shamrock Aluminium Manufacture of a paste of non-leafing aluminium flake pigment incorporating a metal soap
DE19501307C2 (de) * 1995-01-18 1999-11-11 Eckart Standard Bronzepulver Farbige Aluminiumpigmente, Verfahren zu deren Herstellung sowie deren Verwendung
US6933331B2 (en) 1998-05-22 2005-08-23 Nanoproducts Corporation Nanotechnology for drug delivery, contrast agents and biomedical implants
JP4484503B2 (ja) * 1998-04-20 2010-06-16 旭化成メタルズ株式会社 アルミニウム顔料の製造方法
EP1080810B1 (fr) 1998-04-20 2006-06-14 Asahi Kasei Metals Limited Pigment d'aluminium
US6224284B1 (en) 1999-10-12 2001-05-01 Dri Mark Products Incorporated Metallic ink composition for wick type writing instruments
US6855426B2 (en) 2001-08-08 2005-02-15 Nanoproducts Corporation Methods for producing composite nanoparticles
JP4536075B2 (ja) * 2001-09-06 2010-09-01 東洋アルミニウム株式会社 アルミニウムフレーク顔料の製造方法
ES2323948T3 (es) 2001-09-06 2009-07-28 Toyo Aluminium Kabushiki Kaisha Metodo de produccion de pigmento de aluminio en escamas.
JP4610812B2 (ja) * 2001-09-06 2011-01-12 東洋アルミニウム株式会社 アルミニウムフレーク顔料の製造方法
US7708974B2 (en) 2002-12-10 2010-05-04 Ppg Industries Ohio, Inc. Tungsten comprising nanomaterials and related nanotechnology
CN102389977B (zh) * 2003-03-13 2014-07-16 东洋铝株式会社 铝片颜料的制备方法
DE10315775A1 (de) * 2003-04-04 2004-10-14 Eckart Gmbh & Co. Kg Dünne deckende Aluminiumpigmente, Verfahren zur Herstellung derselben und Verwendung der Aluminiumpigmente
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DE102004026955A1 (de) 2004-06-01 2005-12-29 Eckart Gmbh & Co. Kg Wässrige Beschichtungszusammensetzung mit korrosionsstabilen dünnen deckenden Aluminiumpigmenten, Verfahren zu deren Herstellung und Verwendung derselben
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JP2008280405A (ja) * 2007-05-09 2008-11-20 Toyo Aluminium Kk アルミニウム顔料およびその製造方法ならびに該アルミニウム顔料を含む水性メタリック塗料組成物
EP2017310B1 (fr) * 2007-07-17 2014-02-12 Eckart GmbH Encre d'impression à jet d'encre contenant de minces pigments à effets d'aluminium
DE102008029821A1 (de) * 2008-06-25 2009-12-31 Eckart Gmbh Pigmentmischung von PVD-Aluminiumeffektpigmenten und dünnen Aluminiumeffektpigmenten aus Vermahlung, Verfahren zu deren Herstellung sowie deren Verwendung
EP2632994B1 (fr) * 2010-10-29 2018-09-12 Hewlett-Packard Development Company, L.P. Encres électrophotographiques liquides (lep) métalliques et procédés associés
CN104884540B (zh) * 2012-12-28 2017-05-10 东洋铝株式会社 鳞片状铝粉糊剂的制造方法
JP6855378B2 (ja) * 2015-08-14 2021-04-07 旭化成株式会社 アルミニウム顔料、アルミニウム顔料の製造方法、アルミニウム顔料を含む塗料組成物、塗膜、当該塗膜を有する物品、インキ組成物、及び印刷物
JP6982963B2 (ja) * 2017-02-22 2021-12-17 旭化成株式会社 リーフィングアルミニウム顔料、リーフィングアルミニウム顔料の製造方法、リーフィングアルミニウム顔料を含む塗料組成物、塗膜、当該塗膜を有する物品、インキ組成物、及び印刷物
JP6940957B2 (ja) * 2017-02-22 2021-09-29 旭化成株式会社 樹脂付着アルミニウム顔料、塗料組成物、塗膜、塗膜を有する物品、インキ組成物、及び印刷物

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DE102007036369A1 (de) 2007-07-31 2009-02-05 Eckart Gmbh Metallic-Lack, Verfahren zu seiner Herstellung und Verwendungen desselben
US8361217B2 (en) 2007-07-31 2013-01-29 Eckart Gmbh Metallic paint, method for the production thereof, and uses thereof

Also Published As

Publication number Publication date
KR940005837B1 (ko) 1994-06-24
US5127951A (en) 1992-07-07
KR910018498A (ko) 1991-11-30
EP0451785B2 (fr) 1999-03-03
EP0451785A1 (fr) 1991-10-16
DE69110729T2 (de) 1996-04-11
JP2575516B2 (ja) 1997-01-29
CA2039949C (fr) 1995-11-14
DE69110729D1 (de) 1995-08-03
JPH03294360A (ja) 1991-12-25
CA2039949A1 (fr) 1991-10-12
DE69110729T3 (de) 1999-06-17

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